Chemical process.



cNrTnn 'sTATEs PATENT old-Ton.

CHARLES E. PELLEW AND DORRIS W. WHIPPLE, OF NEW YORK, N. Y., ASSIGNORS TO COLUMBIA PROCESS COMPANY, A CORPORATION OF NEW YORK J JZMLABLE COPY Patented April 14, 1908..

CHEMICAL PROCESS. 3,113 i Application filed April 16, 1907. Serial No. 368,593.

To all whom it may concern:

e it known that we, CHARLES E. PELLEW and Donnrs W. I I-IIPPLE, citizens of the United States, and residents of New York city, county, and State, have invented certain new and useful Improvements in Chemical Processes, of which the following is a full, clear, and exact description, such as will enable others skilled in the art to which it appertains to carry out the same.

his invention relates broadly to the art of effectuating chemical reactions, but, more specifically it concerns various improvenature as to be capable of being readily car ried out by any person skilled in the art to accomplish the purposes intended.

Other objects and advantages will be in part obvious and in part pointed out herein after.

This invention accordingly consists in the several steps and the relation and order of one or more of such steps with relation to each of the others thereof which will be exemplified in the process hereinafter described and the scope of the a plication of which will be indicated in the f0 lowing claims.

To facilitate a better understanding of the character and commercial importance of the hereinafter described embodiment of this invention, it may here be noted that tetrachlorid of tin, although heretofore conimercially available mainly in the form of a solution of uncertain purity and strength, is very extensively usec especially in the textile arts as a mordant. The commercial production of a pure crystalline stannic chlorid hydrate has, however, been accomplished at a reasonable price, although such a product would be with a given compound, While in a fluid dissolved state, through the instrumentality of certain catalytic agents. Since, however, certain advantages characteristic of this in vention prominently appear when it is resorted to for the pur )ose of producing tetrachlorid of tin, it will be conducive to clearness to disclose it in such relation.

ne object of this invention is to formulate a commercially practical method especially adapted to be continuously carried out for the purpose of changing the com osition of certain substances, while in a fuse( or dissolved state or in the form of an emulsion, by subjecting such substances to the action of a gaseous element and by promoting reaction with a peculiar catalytic agent.

Another object within the contemplation of this invention is to subject a metal or its salts to the action of one or more members of the halogen group, in such a manner and in the presence of such other elements or con1- pounds as will cause a reaction to readily take place under the control of the operating chemist.

their various operations, with a concomitant saving of expense.

In carrying out our process, we may start either with metallic tin or with a salt thereof, depending upon which is the most readily available om a commercial standpoint.

d are subject with the many which our process diverse conditions under may be carried out.

which a substance such orm ASSUDHDO that we desire to obta1n as mercuric chlorid may be employed in a solid or crystalline tetra-chlorid of tin concatalytic capacity to promote the combinataining water of crvstalhzation as repretion of the chlorin with the tin.

This invention in general seeks to provide a process of the nature described which, from a commercial standpoint, will in practice possess a high degree of efficiency and which, chemically considered, will be of the greatest possible simplicity, being composed of but few steps, all adapted for being performed at I a minimum of cost, and individually of such sented by the formula SnOl .5I-I O, this granular tin will be put in a suitable vessel containing about 200 cc. of water or a solu- SnCl A small quantity of the catalytic agent will also be added and for this purpose about 1 gram of either metallic mercury or an equivalent or mercuric chlorid may be used. Ohlorin gas, evolved in a suitable generator, will be led through a non corrosive tube, as of glass, and passed into the water containing the tin and mercury. A series of reactions will at once take place causing a dissolution and ultimate conversion of the tin into stannic chlorid. The chlorin acts upon the metallic mercury and converts it into mercuri chlorid in accord ance with this reaction: H ;+Cl --l*IgCl and the resultant mercuric chlorid then successively acts on the tin, first converting it to stannous chlorid and then into stannic chlorid as follows:

Sn HgGl SnCl Hg SnCl HgCl S1101, Hg

These reactions will continue to take place so long as any of the metallic tin remains undissolved, and ultimately all the mercury will be held in solution as the mercuric chlorid and the tin as the stannic chlorid. The same end may be obtained by starting wit h a solution of stannous chlorid, which preferablyg hguld be super-saturated and may ad vantageously be prepared from tin salt which is of the composition expressed by the formula SnCl SZH O by mixing 100 grams of the salt with about 25 cc. of water and stirring up into an emulsion or mush. To this mush will be added about 1 gram of mercuric chlorid and the chlorin gas will then be assed through this mixture, which will immediately become heated by the reactions, forming a solution around the chlorin conveying tube, until ultimately the whole will be in solution after about 30 grams of gas has been used. This solution, like that of the preceding embodiment of this invention, contains the tin as a stannic chlorid and the mercury as a mercuric chlorid. The reactions are substantially the same with the exception that here the action begins on stannous chlorid, while there the action begins on metallic tin which is initially converted to the stannous chlorid. It is also to be understood that this invention may be carried out by melting the basisof the reaction. Thus we fuse the stannous chlorid which occurs in the trade in the form of colorless trans aarent deliquescent crystals (commonly called tin crystals). If we desire to obtain the stannic chlorid in the form of cystals containing considerable water of crystallization, we prefer to add a small amount of water to the fused tin crystals to enable the following reaction to ensue:

SnOl 2-H O 01, iro sncusrro This reaction also takes place in the solutions mentioned in the two preceding adaptations of this invention.

The separation of the stannic chlorid from the mother liquor containing the mercuric chlorid can be very easily accomplished by allowing the solution to cooluntilthe stanni clil orid crystallizes out. These crystals the contain considerable Water of crystallization as represented by the formula Sn cusrno.

from the mother liquor in a centrifugal machine or other straining means.

l/Vh1le various substances mlght be employed tions of this invention, mercury and the adapted in practice for the tetra-chlorid of tin owi as a catalytic agent in certain adaptawe have found that salts thereof are peculiarly production. of ng to the readiness with which the several reactions take place. It will thus be perceived that, as a result of our exhaustive experiments and extensive investigations, we have discovered a peculiar treatment, with which been able to devise an and commercially satisfactory metho as a basis We have inexpensive, simple dof continuously manufacturing tetra-chlorid of tin, either in the form of crystals of great purity, or as a solution of any desired strength.

this method, we may dues of tin for the purpose of treat various resiconvertmg the latter into the tetra-chlorid and this method can accordingly be utilized with great economy by the textile industries.

As our process could various ingredients and be carried out with steps without departing from the spirit or scope of our invention, we intend that all matter contained in the above description shall be interpreted in an illustrative rather than in a limiting sense.

We also desire it language used tended to cover all the features of the herein and all statements of the as a matter of language, therebetween.

Having thus disclosed to be understood that the in the following claims is ingeneric and specific disclosed invention, scope thereof which, might be said to fall our invention, What we claim and desire to secure by Letters Patent of the United States is:

1. The art of promoting a chemical reaction consisting in treating a metal or salt thereof with a reactive substance in the presence of a mercurial catalytic agent.

tion consisting in treat catalytic agent.

in the presence of a agent.

2. The art of promoting a chemical reacing a metal or salt thereof with an acid-forming element or compound thereof in the presence of a mercurial 3. The art of promoting a chemical reaction consisting in treating a metal or salt thereof with a halogen or compound thereof mercurial catalytic 4. The art of promoting a chemical reaction consisting in treating a metal or salt thereof with chlorin or in the presence of a agent.

a compound thereof mercurial catalytic 5. The art of promoting a chemical reac tion consisting in treating a metal or salt thereof with chlorin gas in the presence of a mercurial catalytic agent.

6. The art of promoting a chemical reaction consisting in treating a quadrivalent metal or salt thereof with a reactive substance in the presence of a catalytic agent.

g a quadrivalent metal or salt thereof with an acid-forming element or compound thereof in the presence of 'a catalytic agent.

8. The art of promoting a chemical reaction consisting in treating a quadrivalent metal or salt thereof with a halogen or compound thereof in the presence of a catalytic agent.

9. The art of promoting a chemical reaction consisting in treating a quadrivalent metal or salt thereof with chlorin or a compound thereof in the presence of a catalytic agent.

10. The art of promoting a chemical reaction consistin in treating a quadrivalent tal or salt thereof with chlorin gas in the presence of a catalytic agent.

11. The art of promoting a chemical reaction consisting in treating tin or a salt thereof with a reactive substance in the presence of a catalytic agent.

12. The art of promoting a chemical reaction consisting in treating tin or a salt thereof with an acid-forming element in the presence of a catalytic agent.

. 13. The art of with a halogen or compound thereof in the presence of a catalytic agent.

14. The art of producing consisting in treating tin with chlorin or a compound thereof in the presence of a catalytic agent.

15. The art of stannic chlorid 16. The art of producing stannic chlorid consisting in treating metallic tin with a reactive substance in the presence of a catalytic agent.

17. The art of promoting a chemical reaction consisting in treating metallic tin with a alogen or compound thereof in the presence of a catalytic agent.

18. The art of producing stannic chlorid consisting in treating metallic tin with chlorin or a compound thereof in the presence of a catalytic agent.

19. The art of producing stannic chlorid consisting in treating a dissolved tin salt with chlorin or a compound thereof in the presence of a catalytic agent.

20. The art of promoting a chemical reaction consisting in treating a melted metal or salt thereof with a reactive substance in the presence of a catalytic agent.

" salt thereof 21. The art of promoting a chemical reaction consisting in treating a melted metal or with an acid-forming element in the presence of a catalytic agent.

22. The art of promoting a chemical reaction consisting in treating a melted metal or salt thereof with a halogen or compound thereof in the presence of a catalytic agent.

23. The art of promoting a chemical reaction consisting in treating metallic tin with a reactive substance in the presence of a fluidv and a catalytic agent.

24. The art of promoting a chemical reaction consisting in treating metallic tin with a halogen or compound thereof in the presence of a fluid and a catalytic agent.

25. The art of producing stannic chlorid consisting in treating metallic tin with chlorin or a compound thereof in the presence of water and a catalytic agent.

26. The art of promoting a chemical reaction consisting in treating a solution of a presence of a catalytic agent.

27. The art of promoting a chemical reacof a catalytic agen 30. The art of promoting a chemical reaction consisting in treating a solution of a tin salt with a halogen or compound thereof in the presence of a catalytic agent.

31. The art of producing a stannic chlorid consisting in treating a solution of a tin salt with chlorin or a compound thereof in the presence of a catalytic agent.

32. The art of presence of a catalytic agent.

33. The art of promoting a chemical reaction consisting in treating a solution of stannous chlorid with a halogen or compound thereof in the presence of a catalytic agent.

compound thereof in the presence of a catalytic agent.

35. The art of producing stannic chlorid consisting in treating metallic tin with chlorin gas in the presence of water and a cataconsisting in treating a strong solution of stannous chlorid with chlorin gas in the presence of a catalytic agent.

38. The art of producing solid SnCLbI-LO consisting in treating metallic tin with chlorin gas in the presence of water and a catalytic agent until a solution of stannic chlorid is obtained, and then crystallizing out the stannic chlorid.

39. The art of producing solid SnCl .5H O consisting in treating fused hydrated stannous chlorid with chlorin gas in the presence of a catalytic agent, and then crystallizing out the stannic chlorid.

40. The art of producing solid 51101 511 0 consisting in treating a strong solution of stannous chlorid with chlorin gas in the presence of a catalytic agent, and crystallizing out the formed stannic chlorid.

41. The art of producing solid SnCl .5H O consisting in treating metallic tin with chlorin gas in the presence of water and mercury l or a salt thereof, and then crystallizing out the formed stannic chlorid.

42. The art of producing solid SnCl .5H O consisting in treating fused hydrated stannous chlorid with chlorin gas in the presence of mercury or a salt thereof, and then crystallizing out the formed stannic chlorid.

43. The art of producing solid SnCl .5H O consisting in treating a strong solution of stannous chlorid with chlorin gas in the presence of mercury or a salt thereof, and then crystallizing out the formed stannic chlorid.

In testimony whereof, we affix our signatures, in the presence of the two subscribed Witnesses.

CHARLES E. PELLEW. DORRIS WV. WHIPPLE.

V' itnesses G. WHEELER, ALBERT F. NATHAN. 

